Chinese Journal of Chromatography ›› 2018, Vol. 36 ›› Issue (4): 370-375.DOI: 10.3724/SP.J.1123.2017.11018

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Determination of four hydroxyl polycyclic aromatic hydrocarbons in urine by solid-phase extraction with monolithic column coupled with high performance liquid chromatography

HU Guiyu, WANG Manman, NIAN Qixun, LI Na, DONG Xinxin, HAO Yulan, WANG Qian, WANG Xuesheng   

  1. School of Public Health, North China University of Science and Technology, Tangshan 063000, China
  • Received:2017-11-13 Online:2018-04-08 Published:2014-02-26
  • Supported by:

    National Natural Science Foundation of China (No. 21305028); Natural Science Foundation of Hebei Province (Nos. H2017209232, H2016209018); Training Foundation of North China University of Science and Technology (No. JQ201717).

Abstract:

A method based on monolithic column solid-phase extraction (SPE) coupled with high performance liquid chromatography (HPLC) was developed for the simultaneous determination of four hydroxyl polycyclic aromatic hydrocarbons (OH-PAHs) in urine.A poly (butyl methacrylate-co-ethylene dimethacrylate) monolithic column was prepared in a syringe and was used as the sorbent.The parameters influencing SPE, such as loading volume, washing solvent, eluent, and elution volume, were investigated in detail.Under the optimized conditions, the linearities were obtained in range of 1.2-200.0 ng/mL, and the LODs and LOQs of the analytes were 0.06-0.09 ng/mL and 0.20-0.30 ng/mL, respectively.The intra-day and inter-day relative standard deviations were 1.4%-5.3% and 2.6%-7.3%, respectively.The recoveries evaluated using the spiked (3 ng/mL) urine samples of coke oven workers ranged from 78.2% to 117.0%.The feasibility of the developed method was further demonstrated for the analysis of the real samples.The results indicated that the reusable monolithic column enabled effective purification and enrichment of the four OH-PAHs in urine, and can be applied to the analysis of OH-PAHs in urine due to its simplicity and accuracy.

Key words: high performance liquid chromatography (HPLC), hydroxyl polycyclic aromatic hydrocarbons (OH-PAHs), polymer monolithic column, solid-phase extraction (SPE), urine

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